反応 #74908

反応方程式

5-chloro-1-indanone

nitric acid

→

5-Chloro-6-nitro-1-indanone

反応条件

後処理

1. 1
   その他remains between -10° and -15° C
2. 2
   workup.ADDITIONAfter the addition
3. 3
   workup.ADDITIONthe reaction solution is poured onto ice
4. 4
   その他the precipitate which has separated out
5. 5
   ろ過is filtered off
6. 6
   洗浄washed with water
7. 7
   その他The crude product of melting point 110°-113° is recrystallized from ethanol, whereby the melting point of the pure 5-chloro-6-nitro-1-indanone
8. 8
   その他rises to 126°-128° C.

実験手順

86.0 g (0.51 mole) of 5-chloro-1-indanone are introduced in portions into 540 ml of fuming nitric acid (d=1.54), cooled to -20° C., so that the temperature of the reaction mixture remains between -10° and -15° C. After the addition has ended, the mixture is subsequently stirred for 45 minutes at -15° to -20° C., the reaction solution is poured onto ice and the precipitate which has separated out is filtered off and washed with water. The crude product of melting point 110°-113° is recrystallized from ethanol, whereby the melting point of the pure 5-chloro-6-nitro-1-indanone rises to 126°-128° C.

出典